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目的:改进现有甲酚及甲酚皂溶液含量测定中各组分均不能完全得以分离的缺陷,建立一个新的气相色谱方法。方法:采用毛细管柱气相色谱法,安捷伦6890型气相色谱仪;安捷伦DB-225毛细管柱,(50%氰丙基苯基)二甲基聚硅氧烷为固定液,长30m、内径0.32mm、膜厚0.25μm。程序升温110℃(31min)20℃.min-1150℃(10min),载气:99.99%氮气,流速1mm.min-1;采用分流进样,进样量1μL。结果:采用毛细管柱气相色谱法能较大地提高组分之间的分离度。甲酚中各组分的线性关系为,邻甲酚:Y=3.77X-0.0087(y=0.9998);对甲酚:Y=3.67X-0.0011(y=0.9996);间甲酚:Y=3.58X-0.0068(y=0.9997)。平均回收率为98.99%,RSD=0.95%(n=9)。结论:本法准确,专属性好,可用作控制甲酚及甲酚皂溶液质量的方法。
Objective: To improve the existing cresol and cresol soap solution of each component can not be completely isolated defects, the establishment of a new gas chromatography method. Methods: The capillary column gas chromatography, Agilent 6890 gas chromatography; Agilent DB-225 capillary column, (50% cyanopropyl phenyl) dimethyl polysiloxane as a fixed liquid, length 30m, an inner diameter of 0.32mm, Film thickness 0.25μm. Programmed temperature was 110 ℃ (31min) 20 ℃ .min-1150 ℃ (10min), carrier gas: 99.99% nitrogen, flow rate 1mm.min-1; using split injection, injection volume 1μL. Results: Capillary gas chromatography can greatly improve the separation between components. Cresol: Y = 3.77X-0.0087 (y = 0.9998); p-cresol: Y = 3.67X-0.0011 (y = 0.9996); m-Cresol: Y = 3.58 X-0.0068 (y = 0.9997). The average recovery was 98.99%, RSD = 0.95% (n = 9). Conclusion: This method is accurate and specific, and can be used as a method to control the quality of cresol and cresol soap solution.